The experiments have been performed to obtain zinc complex compound with smaller particle sizes, which is used as a charge control agent in manufacturing toner. Metallic salts and polyhydric alcohols have been studied to investigate their effects on the formation and the triboelectric charge of zinc complex-compound particle with different sizes. Reactants such as zinc chloride and 3,5-di-tert.-butyl salicylic acid have been used to form the complex compound. Polyethylene glycol (PEG-300), glycerin and ethylene glycol have been added into the zinc chloride solution beforehand to lower the reaction rate in the formation of zinc complex-compound. Aluminium(III) chloride has been mixed in the zinc chloride solution beforehand to restrain the particle size from growing. When PEG-300 and aluminium(III) chloride are used to lower the reaction rate and to restrain the particle size from growing, the average particle size of zinc complex compound decreases from 5.28 μm to 2.33 μm, which was 44.1% of 5.28 μm.